In this study, the sandwich‐like bis(phthalocyaninato)lanthanide(III) complexes MPc2 (M = Lu, Gd) have been prepared. The reaction of 4,5‐bis(mercaptopropylisobutyl‐POSS)phthalonitrile (1) [POSS: polyhedral oligomeric silsesquioxane] with lithium gave the dilithium octakis(mercaptopropylisobutyl‐POSS)phthalocyaninate which was further reacted in situ with Lu(OAc)3·3H2O and Gd(OAc)3·4H2O in 1‐pentanol to give compounds 2 and 3, respectively. The structure of the target compounds was confirmed by elemental analysis, UV/Vis and IR spectroscopic as well as MALDI‐TOF mass spectrometric techniques. The nonlinear absorption andoptical limiting (OL) performance of 2 and 3 are investigated by means of the Z‐scan technique. While 2 exhibits a good nonlinear absorption, 3 possesses a low nonlinear absorption. The ratio of the excited‐state to ground‐state absorption cross sections, κ, the effective nonlinear absorption coefficient, βeff, and the energy density, Fsat, were determined for 2. The results indicated that 2 possesses a good combination of optical limiting parameters.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008)

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